Graphene Oxide (GO)/Polystyrene (PS) nanocomposites of thisckness (50 μm) have been synthesized by solution blending method with DMF as solvent. The composites have been coagulated by drop wise addition of DMF into a large volume of methanol. These composites filled almost completely with graphene oxide (GO) as a filler concentration (0.01–0.5 wt %) by volume. Hydrogen adsorption study on these composites has been performed by sievert’s type apparatus at room temperature. The storage capacity upto 5.02 wt% has been obtained by repetition of various cycles at constant pressure. Dynamic Mechanical Analysis (DMA) has been performed for testing of mechanical strength of these fabricated composites. Storage modulus has been found to be increased at low concentration of graphene oxide in polystyrene matrix. Scanning Electron Microscopy (SEM) has been used for surface morphology of fabricated composites, from SEM micrographs layered structure of graphene oxide has been obtained. The Dielectric constant (up to 5.4) has been found at higher graphene oxide concentration in polystyrene matrix due to interfacial effect and accumulation of charges. From Differential Scanning Calorimetry (DSC) the glass transition temperature (90 °C) at higher concentration of graphene oxide in PS matrix has been obtained. © 2016 American Scientific Publishers. All rights reserved.